流动注射化学发光传感器测定抗坏血酸

基于抗坏血酸抑制ＫＭｎＯ４－鲁米诺体系化光反应这一效应，设计出一种简便，快速，灵敏度高的消耗型化学发光抗坏血酸传感器。该传感器线性响应范围为１．０＊１０＾－５－４．０＊１０＾－３ｇ／Ｌ；相对标准偏差为２．３％（１．０＊１０＾－４ｇ／Ｌ，ｎ＝１１）；     

马来酸麦角新碱化学发光传感器的研究

基于发光试剂通过电价键将铁氰化钾固定在阴离子交换树脂上 ,可直接对待测物马来酸麦角新碱进行传感 ,从而建立测定药物马来酸麦角新碱的传感器新方法。其线性范围为 5× 10 -3 ～ 1mg/L ,线性方程为ΔI =10 6 .4 5C +17.10 (R2 =0 .998) ,检出限达到 2 .6 μg/L。对 0 .0 1和 0 .1mg/L的马来酸麦角新碱进行10次测定 ,它们的相对标准偏差 (RSD)分别为 2 .1%、2 .4 %。此传感器的稳定性良好 ,可连续使用 2 0 0次以上。此法已成功地用于马来酸麦角新碱注射液含量的测定以及尿样中马来酸麦角新碱含量的检测     

A Fluorescence-Based Sensor for Ammonium and Nitrate

Abstract

Measurement of nitrite and nitrate in rain samples was performed using a fluorescence based sensor. Nitrite and nitrate were reduced to ammonia using Devarda's alloy, and the gas was then passed through a membrane and reacted with o-phthalaldehyde. A linear relationship between the nitrate concentration and the luminescence intensity was observed over the concentration range of 1 – 5 mg/1, with a relative standard deviation (RSD) of 2.3% at a nitrate concentration of 1 mg/1 (n = 5). The system did not show any response toward sulfate or chloride. Results obtained from the measurement of river water samples using the sensor showed good agreement with those obtained using a conventional method.     

Chemiluminescence flow system for the determination of ammonium ion

A novel chemiluminescence (CL) system for ammonium ion combined with flow-injection analysis is presented in this paper. It is based on the CL reaction between luminol, immobilized electrostatically on an anion-exchange column, and chlorine electrochemically generated on-line via a platinum electrode from hydrochloric acid in a coulometric cell. Ammonium ion reacts with chlorine and decreases the observed CL intensity. The system responds linearly to ammonium ion concentration in the range 1.0-100 muM, and the detection limit is 0.4 muM. A complete analysis, including sampling and washing, could be performed in 1 min with a relative standard deviation of <6.0%. The system is stable for over 500 determinations and has been applied successfully to the determination of ammonium ion in rainwater samples.     

Enhanced Sensitivity of the Tris(Bipyridine)Ruthenium(II) Chloride Electrogenerated Chemiluminescence Sensor with Porous Silica Nanoparticles

Mass transfer in electrogenerated chemiluminescence affects the sensitivity of sensors involving this technique. Herein, the characteristics of the porous Ru(bpy)₃²⁺/silica nanoparticles were investigated by transmission electron microscopy, fluorescence spectroscopy, ultraviolet-visible absorption spectroscopy, and electrogenerated chemiluminescence. The results showed that the pores inside the porous nanoparticles provided efficient mass transfer, resulting in significant enhancement of electrogenerated chemiluminescence. Consequently, a novel electrogenerated chemiluminescence sensor was developed and is reported herein. The sensitivity for tripropylamine was more than one order of magnitude higher compared to previously reported similar sensors, with a limit of detection of 3.3 × 10^?12 moles per liter.     

联吡啶钌电化学发光传感器测定海洛因

利用离子液体为粘合剂制作碳糊电极,采用高分子聚合法,合成包埋有Ru(bpy)2(dcbpy)2+的高分子聚合物,将钌聚合物掺杂于离子液体碳糊电极中,制作电化学发光传感器.结果表明,此传感器具有很好的电化学发光特性,与用石蜡油为粘合剂制作的电化学发光传感器相比,离子液体为粘合剂的电化学发光传感器检测三丙胺的检出限降低1个数量级.海洛因对电化学发光传感器的发光信号有很好的增强作用,基于此建立了高灵敏度检测海洛因的电化学发光分析法,海洛因浓度与电化学发光信号在2.0×10-9～2.0×10-5 mol/L范围内呈良好的线性关系,检出限为8×10-10 mol/L (S/N=3).将电化学发光传感器在5.0×10-9 mol/L海洛因溶液中采用线性循环电位连续扫描60圈,相对标准偏差小于2.2%.本方法用于血清中海洛因的检测,其回收率为94%～101%.     

一种新型分子印迹聚合物基的化学发光阵列传感器

建立了一种分子印迹-化学发光阵列传感器测定甘氨酸的新方法. 该方法以甘氨酸为模板分子, 合成了分子印迹聚合物微球, 将该聚合物微球固定在96孔板上, 用它来识别丹磺酰氯标记的甘氨酸(Dns-Gly). 最后加入化学发光试剂(TCPO-H2O2-咪唑), 测量相对化学发光强度定量检测甘氨酸. 在最佳试验条件下, 相对化学发光强度和甘氨酸的浓度在0.2～60 μmol/L范围内成良好的线性关系, 相关系数为r＝0.9972, 方法的检出限为0.07 μmol/L, 对1 μmol/L甘氨酸溶液进行11次平行测定, 相对标准偏差为3.3% (n＝11). 由于以甘氨酸为模板分子合成出来的分子印迹聚合物空腔比较小, 避免了非特异性吸附, 使它在识别丹磺酰氯标记的甘氨酸时特异性、响应速度和灵敏度都有所增强.     

Flow—injection Chemiluminescence Sensor for the Determination of Gallic Acid by Immobilizing Luminol and Periodate on Anionexchange Resin

ＩｎｔｒｏｄｕｃｔｉｏｎＧａｌｌｉｃａｃｉｄｅｘｉｓｔｓｉｎｔｈｅｌｅａｖｅｓａｎｄｆｒｕｉｔｓｏｆｍａｎｙｔｙｐｅｓｏｆｐｌａｎｔｓａｎｄｉｓｗｉｄｅｌｙｕｓｅｄｉｎｍｅｄｉｃｉｎｅｆｏｒａｎｔｉ ｏｘｉ ｄａｔｉｏｎａｎｄａｎｔｉｂａｃｔｅｒｉａｌａｃｔｉｖｉｔｙ ,ａｎｔｉｆｌａｍｍａｔｏｒｙａｃｔｉｏｎａｎｄａｎｔｉ ｃａｎｃｅｒａｃｔｉｖｉｔｙ .1 5Ｉｎｓｐｉｔｅｏｆｔｈｅｈｅａｌｔｈｉｍｐｏｒｔａｎｃｅｏｆｇａｌｌｉｃａｃｉｄ ,ｉｔｓｍｅｔａｂｏｌｉｓｍａｎｄｋｉｎｅｔｉｃｓｉｎｔｈｅｈｕ…     

Chemiluminescence determination of atenolol in biological fluids by a europium-sensitized permanganate-sulfite system

A simple flow injection chemiluminescence (CL) method was developed for the determination of atenolol using Eu³⁺ as the probe. It was found that the weak CL generated by the KMnO₄-Na₂SO₃ reaction can be significantly enhanced by the atenolol-Eu³⁺ complex. The experimental conditions were optimized. The CL intensity was linearly related to atenolol concentration in the range from 8.0 × 10⁻⁹ to 1.0 × 10⁻⁵ g mL⁻¹. The detection limit (3s _b) was 3 × 10⁻⁹ g mL⁻¹ and the relative standard deviation for 1.0 × 10⁻⁷ g mL⁻¹ atenolol solution was 2.4% (n = 11). The method has high sensitivity, wide linear range, inexpensive instrumentation, and has been applied to the determination of atenolol in spiked human urine and plasma samples with recoveries within the range 95.5–104.0%. Supplementary material to this paper is available in electronic form at Electronic supplementary material: Discussion of the reaction mechanism and additional figures are available online as electronic supplementary material (ESM) at . Correspondence: Jianxiu Du, Key Laboratory of Analytical Chemistry for Life Science of Shaanxi Province, School of Chemistry and Materials Science, Shaanxi Normal University, Xi’an 710062, P.R. China     

Determination of Tetracyclines in Milk with a Molecularly Imprinted Polymer-Based Microtiter Chemiluminescence Sensor

A molecularly imprinted polymer (MIP) capable of recognizing five tetracyclines using minocycline as the template was synthesized for the first time. The MIP was employed as the recognition reagent to prepare a chemiluminescence sensor on a conventional microtiter plate. The light signal was initiated using the highly efficient bis(2,4,6-trichlorophenyl) oxalate-hydrogen peroxide-imidazole chemiluminescence system. After optimization of several appropriate factors, the sensor was employed to determine five tetracyclines in milk. The developed assay contained only one sample-loading step, so each measurement was completed within 12?min. The limits of detection for these analytes were in the range from 0.5 to 2.0?pg/mL, while the recoveries from the fortified milk samples were between 78.1 and 105%. In addition, the sensor was shown to be reusable for up to four measurements. Hence, this sensor has been demonstrated to be a simple, rapid, sensitive, and durable tool for the determination of tetracyclines in animal-derived food.     

Immobilized and solid-state reagent systems for luminol chemiluminescence in flow systems

To facilitate the application of luminol chemiluminescence in analysis, several approaches are investigated to provide the reagents in immobilized or solid-state format. The approaches are demonstrated with flow injection systems. Luminol is covalently bound or adsorbed to the surface of small support particles and packed into flow-through reactor/detector cells. The catalyst can be either covalently immobilized heme-containing species or a positively-biased electrode in an electrochemical cell. Peroxide can be obtained electrochemically at a negatively-biased electrode. These immobilized reagent systems can be combined to yield single-channel flow systems for determination of hydrogen peroxide (0.15M detection limit) or luminol (0.1 nM detection limit).     

A PVC-based 1,8-diaminonaphthalen electrode for selective determination of vanadyl ion

A PVC membrane vanadyl (VO²⁺) ion-selective electrode was constructed using 1,8-diaminonaphthalen (DAN) as a neutral carrier. The electrode shows good Nernstian response for VO²⁺ ions over a wide concentration range (1.0×10⁻¹-1.0×10⁻⁵ M). The optimum composition of the membrane was 55 wt.% poly(vinylchloride), 35 wt.% 2-nitrophenyl octyl ether (NPOE), 5 wt.% ionophore, and 5 wt.% potassium tetrakis(p-chlorophenyl)borate (KTpClPB). It has relatively fast response time and can be used at least for 5 weeks without any considerable divergence in potentials. The proposed electrode revealed relatively good selectivity for VO²⁺ over wide variety of other metal ions. The electrode was used for the potentiometric titration of VO²⁺ ions with EDTA.     

基于CoFe2O4表面催化发光的硫化铵气体传感器研究

基于铁酸钴(CoFe₂O₄)纳米材料催化硫化铵的氧化反应产生化学发光的现象, 建立了一种检测空气中痕量硫化铵的催化发光气体传感器. 在对合成的3种材料的催化发光性质进行比较的基础上, 对分析方法条件进行了优化, 其结果表明: 在检测波长400 nm、反应温度306 ℃、载气流速400 mL/min的最优条件下, 可测定的硫化铵浓度的线性范围为0.13～13 mg/L (r＝0.9951, n＝9), 检出限为0.04 mg/L (3σ), 对1.3 mg/L的硫化铵连续平行测定8次, 其相对标准偏差为1.8%. 此外, 考察了相同浓度的常见挥发性有机物的干扰情况, 其结果表明该传感器具有很好的选择性. 连续60 h通过1.3 mg/L的硫化铵, 发光强度无明显降低, 相对标准偏差小于5%, 表明此传感器使用寿命长. 并将该传感器成功用于人工合成样品的分析, 回收率为94.7%～103.9%.     

流动注射化学发光法测定尼莫地平

利用尼莫地平对ce（Ⅳ)-Na2SO3化学发光体系的抑制作用,建立了流动注射—化学发光法测定尼莫地平的新方法。化学发光强度与尼莫地平浓度在0．5～90mg/L范围内呈线性关系,线性范围为0．5～10mg/L时,r=0．9990;线性范围为10～90mg/L时,r=0．9968。回收率在98．3％～103．2％范围内;检出限为0．085mg/L。     

Chemiluminescence flow system for the determination of sulfite

A novel chemiluminescence(CL) flow system for sulfite is described based on electrostatically immobilized luminol on an anion exchange column. Sulfite is detected by the CL reaction with luminol bleeding from the column by hydrolysis. The calibration graph is linear in the range 3 × 10^–7 to 1 × 10^–5 mol/L, and the detection limit is 1 × 10^–7 mol/L. Interfering metal ions co-existing in sample solutions could be effectively eliminated on-line by an upstream cation exchanger. A complete analysis could be performed in 1 min with a relative standard deviation of less than 5%. The system could be reused for over 50 h and has been applied successfully to the determination of sulfur dioxide in air. Received: 21 October 1997 / Revised: 23 February 1998 / Accepted: 26 February 1998     

反相流动注射胶束增敏化学发光分析法测定硝苯地平

基于胶束介质中硝苯地平对碱性鲁米诺-过氧化氢化学发光体系的增敏作用,结合反相流动注射技术,建立了流动注射化学发光分析法测定硝苯地平的新方法.硝苯地平浓度在3.5×10-10～4.0×10-8 g·mL-1范围内时,化学发光强度与硝苯地平的浓度呈良好的线性关系,其相对标准偏差为1.4%(n=11,c=3.5×10-9 g...     

反相流动注射-化学发光法测定氢化可的松

在碱性介质中,氢化可的松可被Fe(CN)6^3-氧化产生化学发光,奎宁对此发光反应有显著的增敏作用。据此,建立了反相流动注射-化学发光法测定氢化可的松的新方法。方法的线性范围和检出限分别为0．05．-50mg／L和0．02mg／L,相对标准偏差(n=11,C=1．0mg／L)为0．9％。方法用于药物中氢化可的松含量的测定,结果与标准方法分光光度法测定结果吻合。     

Chemiluminescence flow system for the determination of sulfite

A novel chemiluminescence(CL) flow system for sulfite is described based on electrostatically immobilized luminol on an anion exchange column. Sulfite is detected by the CL reaction with luminol bleeding from the column by hydrolysis. The calibration graph is linear in the range 3 × 10^–7 to 1 × 10^–5 mol/L, and the detection limit is 1 × 10^–7 mol/L. Interfering metal ions co-existing in sample solutions could be effectively eliminated on-line by an upstream cation exchanger. A complete analysis could be performed in 1 min with a relative standard deviation of less than 5%. The system could be reused for over 50 h and has been applied successfully to the determination of sulfur dioxide in air.     

反相流动注射化学发光法测定葡萄糖

提出使用葡萄糖增强Ｌｕｍｉｎｏｌ－Ｋ７Ｃｕ（ＩＯ６）２－ＫＯＨ化学发光体系，结合高灵敏度的反相流动注射技术进行葡萄糖的测定。本法不仅节省试剂，而且操作简单，重复性好。葡萄糖在４×１０－７～８×１０－５ｍｇ／Ｌ浓度范围内与化学发光分析信号呈线性关系；检出限为１．８Ｘ１０－７ｍｇ／Ｌ；ＲＳＤ＝２．０４％。     

基于纳米银对鲁米诺-铁氰化钾化学发光体系的增敏作用测定硫酸特布他林

基于纳米银对鲁米诺-K3Fe(CN)6化学发光体系的显著增敏作用,建立了流动注射化学发光检测硫酸特布他林的新方法.运用透射电子显微镜(TEM)对所制备的纳米银进行了表征.化学发光光谱和紫外吸收光谱显示将纳米银注入鲁米诺-K3Fe(CN)6体系后,未生成新的发光物质.考察了鲁米诺,K3Fe(CN)6,NaOH以及纳米银浓度对化学发光体系的影响,在优化的实验条件下,该方法对硫酸特布他林检测的线性范围是1.0×10-9～2.0×10-5 g/L(r=0.9935),检出限为1×10-10 g/L,相对标准偏差为3.6%(C=1.0×10-6 g/L, n=11).本方法应用于硫酸特布他林片剂含量的测定,回收率为98.5%～102.5%,并与药典方法进行了比较,结果基本一致.